Black sulfur dye and process of making same.



N TE STATES PATENT OFFICE.

c'usmv EDWARD JUNIUS, or menu, GERMANY, ASSIGNOR T0 n. B. SANDERSON, or NEW YORK, a1. jr.

BLACK SULFUR DYE AND PROCESS OI: MAKING SAME.

Specification of Letters Patent.

Patented 00am. loos.

s mmon flledOctober 24, 1900. Serial No. 340,305. (s ecimens) NiUs, asub'ect of the German Emperor, and.

resident o Hagen, Westphalia, Germany,

Bahnhofstrasse 29, have invented acertain new and useful Black S lfur Dye and Process forManutacturing the Same, 'of.-which the following s a specification.

. I have found that if nitrosoorthocrcsol' (C .H .Cl l .NO.OH. is boiled with sulfid of so ium and sulfur 1n the'presence of water water.

.to boiling point and kept boiling vuntil the a black sulfur dye is formed. Example: 7- arts of' nitrosoorthocresol are 'mixed wit 4 parts of sulfur and about arts of cold The mixture then s owlvv heated li uor assumes a greenish-blue aspect; this tiilres about 24 hours. The Volume of liquor is kept. constant eith" )y condensing the vapor that would otherwise escape and "allowing it to flow-back into the apparatus or by a'suplply of fresh water to compensate for. -that{,w ich evaporates. When the reaction is completed the solution may be used as a dye in the condition in which it then is;

for the dye-solution ma be evaporated to or'the dye-Stu may be isolated by precipitation by anacid or by air or otherwise. The quantities of the aboveexample reduce a color which on cotton gives a lack of a bluish shade greenish-blue shades ofblack may be obtained b increasing the ivalent to"fireplace;part of the so: dium su ate ofan alkali.

. ,Part of the may be carried out at a a higher temperature in the form of what istiachnically known as a melt, but in'every "case Water must be present at the commencement and. the temperature must be low, as otherwise a decomposition of the nitrosoortho-cresol' might take place. However I gets]- the boilin process as I find it gives a ttcrshade. i y this process the d fllcult manufacture ofilamidoortliocrosol' as an. ISO- vlated intermediate product is dispensed with and Wblaokis obtained which dyes cotton dirovt'and which does not require an oxidation after-treatment with chromates or other wise.

In dyes by tliis propagatorthermore, it is necessary to use a'n'itroso- 14 parts of crystallized sodium sulfid,

.me, and notably than the products known as T extra, immediate black NB; vidalblack 438' and generally blacks made from dinitro henol.

pecially fast products are obtained by dividing the sulfuration into two parts; for; instance by making first with little sulfur andsulfid a violet. roduct which is afterwards purified by reclpitating with acid and washmg and is t ion treated again with sulfur and sulfid. Large quantities of sulfur and sulfid can be used in this case. v However, it is advisable not to dry down the dye-solution but to isolate the coloring matter by me cipitatin .either with acid or with a current of air q wn through its solution. thus precipltated and. purified dye-stud has the following properties: It is insoluble in water, acids and alkali carbonates, but is soluble in alkali-sulfids, suchas sodium sulfid. It dyes cotton directly in a bath containing sodium sulfid and salt. The dyeings are fast to light, milling and alkalis, acids and cross dyeing." t

I claim, I I The process of preparing a black d estufi' which consists in treating nitrosoortliocresol with sodium su'lfid and sulfur in the presence of water substantially as described.

2. The .dyestu formed by treating nitroso-o rth0-cresol with sodium sulfid and sulfur inthe resence of water and characterized in the iso andpurified'state by being in-' soluble in water, acids and alkali carbonates; but soluble in alkali, sulfid, such as sodium sulfid; mu bydyeing cotton directly in a bath-containing sodium sulfid and salt, sub- M stantially as described.

The process of preparing ablack dye- The 100 stuff which consists in boiling a bath of water containing nitroso-ortho-cresol, sodium sul- I as described.

id and sulfur, substantially have signed my In testimony whereof name to this specification in the two subscribing witnesses.

GUSTAV EDWARD JUNIUS.

Witnesses: a Jumus,

presence of 

